Journal of Chemical Technology and Biotechnology J Chem Technol Biotechnol 79:533–539 (online: 2004)

DOI: 10.1002/jctb.1021

Evaluation of a simple batch distillation

process for treating wastes from
metalworking industries
P Cañizares, J Garcı́a-Gómez, F Martı́nez and MA Rodrigo∗
Departamento de Ingenierı́a Quı́mica, Facultad de Ciencias Quı́micas, Universidad de Castilla La Mancha, Campus Universitario s/n, 13071
Ciudad Real, Spain

Abstract: A simple batch distillation process for the treatment of two types of industrial waste generated
in a metalworking factory has been evaluated. Both types of waste are oil-in-water emulsions composed of
numerous compounds and each type has a high content of water-soluble species. The water-soluble nature
of the wastes precludes the use of conventional treatment technologies, such as ultrafiltration or chemical
emulsion breaking, since they need to be complemented with additional treatment processes that would
probably increase the cost considerably. A simple characterization of the liquid–vapour equilibrium and
a scale-up study has demonstrated the applicability of this technology. The process allows 90% of the
waste to be recovered as water, thus achieving the required quality limits for discharge into a municipal
wastewater treatment plant. An approximate estimation of capital investment and operating costs for an
existing case has shown the economic viability of this process.
 2004 Society of Chemical Industry

Keywords: distillation; metalworking wastes; emulsions; waste treatment

1 INTRODUCTION semipermeable membrane that only allows water to

Metalworking industries generate oily wastewater
that contains stable oil-in-water emulsions. These
wastewater contaminants arise from the residues of
emulsions that serve the purposes of lubrication,
cooling, surface cleaning and corrosion prevention
in the manufacturing process.
Appropriate treatment of these wastewaters is nec-
essary in order to reduce the impact of the discharge
of such materials into municipal sewage treatment
plants. Several processes have been described in the
literature for the treatment of such waste, but the most
commonly used are chemical de-emulsification,1,2
electrocoagulation3 and ultrafiltration.4 – 8
Chemical de-emulsification is a physico-chemical
process that involves two stages. The first stage consists
of the addition of treatment chemicals (including
acids/bases, coagulants and organic polymers) to break
down the emulsion and the second stage involves
gravity separation (sedimentation or dissolved-air
flotation). Electrocoagulation achieves the same
results as chemical de-emulsification by introducing
some of the reagents required to break down
the emulsion by means of the electrodissolution
of an anode material, which is normally iron or
aluminium sheets. Ultrafiltration is an alternative to
the two treatments described above and employs a
pass through. This process physically separates oil
from an oil–water emulsion.
These treatments can remove most free and
emulsified oil from the waste but, unfortunately,
soluble organic matter contained in the waste can
still be present in high concentrations. For this reason,
some sort of additional treatment must be undertaken
in order to reduce the contamination to acceptable
levels. These additional treatments often consist of
chemical oxidation processes that markedly increase
the treatment cost (in some cases this increase can
be more than the cost of the original separation
treatment). Less expensive biological processes9 – 11
are rarely used since the effluents generated in this
kind of process usually contain biocides to prevent
degradation of the industrial fluids.
In this context, distillation represents a promising
technique for the treatment of these wastes despite
the high cost associated with it. Distillation is a well-
understood operation as it is the most commonly
used technique for the separation of binary and
multicomponent liquid mixtures in the chemical
industry.12 – 15 In the recent literature, however, there
have not been any reports describing the application
of this technology to the treatment of waste flows
generated in metalworking industries, despite the fact

∗ Correspondence to: MA Rodrigo, Departamento de Ingenierı́a Quı́mica, Facultad de Ciencias Quı́micas, Universidad de Castilla La
Mancha, Campus Universitario s/n, 13071 Ciudad Real, Spain
E-mail: Manuel.Rodrigo@uclm.es
(Received 15 July 2003; revised version received 4 December 2003; accepted 17 January 2004)

 2004 Society of Chemical Industry. J Chem Technol Biotechnol 0268–2575/2004/$30.00 533

P Cañizares et al

that some existing plants use this technique for the

treatment of wastewaters generated in a range of
different factories.
The work described here concerns the technical
and economic viability of simple batch distillation
for the treatment of two existing wastes produced in
metalworking industries.

2 MATERIALS AND METHODS

2.1 Analytical procedures
A number of chemical analyses were carried out
to characterize wastes and to evaluate the perfor-
mance of the treatment process. Chemical oxygen
demand (COD) was determined using a HACH
DR200 analyser (method 8000). Carbon concentra-
tions were monitored using a Shimadzu TOC-5050
analyser. Conductivity was measured using a GLP
31 CRISON conductimeter. pH was measured using
a GLP 21 CRISON pH meter. Viscosity was mea-
sured using a CANNON FENSKE 34200 size 200
Opaque Viscometer in a Zoetermer-Holland TAM-
SON thermostatically controlled bath. Turbidity was
measured using a 115 VELP SCIENTIFICA Tur- Figure 1. Experimental set-up used in the laboratory-scale study.

bidimeter. Oil contents were measured gravimetri-

cally by extraction with 1,1,2-trichlorotrifluoroethane
(Partition-Gravimetric Method 5520.B).16 The pres-
ence of demould agents was detected and quantified
by gas chromatography. Solids were measured by a
standard gravimetric technique.

2.2 Laboratory-scale assays

The characteristics of the vapour–liquid equilibria
were evaluated by conducting a number of exper-
iments in the laboratory-scale plant represented in
Fig 1. This equipment consisted of a round-bottomed
flask connected to a condenser and a Dean–Stark
apparatus to collect distilled samples. Samples were
heated by means of a blanket-heating apparatus. The
temperature of the system was continuously monitored
by a thermocouple. A vacuum pump was also fitted to
enable operations in the pressure range between atmo-
spheric pressure and 300 mm Hg (a mercury pressure
gauge was used to measure the operating pressure).
2.3 Pilot-plant assays
Changes in the results caused by scale-up of the system
were evaluated by performing several experiments in
the pilot plant represented in Fig 2. This installation
works under batch operation conditions and consists
of an electrically heated reboiler, a condenser, a
vacuum pump, and a round-bottomed flask in which
the distillate is collected. The capacity of the feed
container (reboiler) was 200 dm3 . The vacuum pump
enables operations to be carried out below atmospheric
pressure and pressures as low as 70 mm Hg were
attained in the system. A thermocouple and a
mercury manometer were used to measure operating
temperatures and pressures, respectively.
Figure 2. Experimental set-up used in the pilot plant-scale study.
3 EXPERIMENTAL RESULTS AND DISCUSSION
3.1 Waste characterization
The work described here concerns the treatment of
wastes generated in a metalworking factory (which
produces ZAMAK and aluminium pieces by cast and
mechanization processes). Two different waste flows
are generated in the processes under investigation.
One waste flow is obtained daily and comes from
the liquid used to cool and remove pieces from the
mould (effluent 1). The second waste flow is generated
bimonthly and arises from the exhaustion of the cutting
oil fluid used in the mechanization process (effluent
2)—this residue is partially contaminated with effluent
1. The expected compositions of both waste flows
are shown in Table 1 and the data were obtained
by a simple mass balance in relation to the factory
process. This simple mass balance does not take into
account solid materials (metal chips created during

534 J Chem Technol Biotechnol 79:533–539 (online: 2004)

 Treatment of wastes from metalworking industries

Table 1. Composition of the two wastes as determined by simple mass balance for the process

Composition (%)

Componenta Description (from commercial data sheets) Effluent 1 Effluent 2

Water 95.36 93.50

Demould agent Aqueous wax and oil emulsion (normal boiling point 100 ◦ C) 1.28 0.25
Lubricant oil Complex formulation of saturated hydrocarbons (C15 –C50 ), antioxidant, 0.09 0.02
anticorrosive, and antifoaming agents (normal boiling point >400 ◦ C)
Hydraulic oil 1 Water/glycol solution with anticorrosive additives (normal boiling point 2.35 0.46
>100 ◦ C)
Hydraulic oil 2 Refined paraffin mineral oil, antioxidant, anticorrosive and antifoaming 0.91 0.18
additives (normal boiling point >300 ◦ C)
Grease paste Refined mineral oil paste, synthetic wax, graphite and other inorganic 0.01 0.02
lubricants (normal boiling point >350 ◦ C)
Cutting oil 1 Refined paraffin mineral oil, glycol, bactericides, non-ionic tensoactive — 4.96
agents, corrosion inhibitors (normal boiling point not specified)
Cutting oil 2 Mineral oil, surfactants and inhibitors (normal boiling point >300 ◦ C) — 0.61
a Commercial product names are intentionally omitted.

the mechanization process) and vaporization (in the
cast process), and so it can only be considered as a
first approximation for the waste composition.
It can be observed that the wastes contain numer-
ous compounds with different characteristics and that
a significant proportion of water-soluble compounds
is present (corresponding to demould agents and
hydraulic fluids). This situation means that a single
conventional method (eg de-emulsification, ultrafil-
tration, electrocoagulation) cannot be used to obtain
a satisfactory treatment since these methods do not
remove water-soluble contaminants. A combination of
treatment techniques (one for splitting oil and water,
and another to remove water-soluble contaminants
from the aqueous waste) or a ‘non-conventional’ (ie
specific to this application) treatment process must
therefore be used. In this sense distillation represents a
promising technique for the treatment of these wastes.
The results of a more exhaustive characterization
of the wastes based on chemical analysis are shown
in Table 2. It can be seen that both waste flows have
high COD values (the parameter used to quantify
the organic matter concentration) and oil contents
as the most significant contaminant parameters. The
data relating to the soluble COD are also given
in Table 2 and these are the best results obtained
from a number of jar-test assays carried out with
different concentrations of various emulsion-breaking
compounds. It can be observed that a conventional
treatment alone cannot be used for processing these
wastes since high COD values are found for the
treated wastes due to the presence of the water-
soluble compounds.
3.2 Laboratory-scale study
From the chemical point of view, both of the industrial
wastes under investigation can be interpreted as
complex multicomponent systems. In fact, a wide
variety of compounds is present in both wastes and
therefore a simple liquid–vapour characterization of
the two systems using standard techniques must
be considered unsatisfactory. Given this situation,
characterization of the system requires a procedure
similar to those used for oils.17 Batch tests were
performed on samples of both wastes and the resulting
system temperature and COD were measured.
The evolution of temperature as a function of the
percentage of distilled waste in the distillation of
effluents 1 and 2 is shown in Figs 3 and 4, respectively,
for three different operating pressures (300, 450 and
700 mm Hg).
As one would expect, low pressures lead to lower
boiling points for the treated wastes. Likewise, it
can be observed that the temperature evolution

Table 2. Average composition of the two industrial effluents studied

Parameter Effluent 1 Effluent 2

Oils (%) 4.64 5.59

pH 5.16 8.80
Conductivity/µS cm−1 813 2805
Density/kg m−3 1095.1 1104.4
Viscosity30 ◦ C /cSt 2.6515 2.2948
COD/mg dm−3 51 500 66 150
Soluble COD/mg dm−3 45 400 6 200
Total carbon/mg dm−3 17 100 17 680 , 700 mm Hg , 450 mm Hg , 300 mm Hg
Solids/mg dm−3 889.2 2518.0
Turbidity/NTU 4 515 12 207 Figure 3. Temperature evolution in the simple batch distillation of
effluent 1.

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P Cañizares et al
, 700 mm Hg , 450 mm Hg , 300 mm Hg
Figure 4. Temperature evolution in the simple batch distillation of
effluent 2.
has three clearly defined stages regardless of the
operating pressure:
The first zone is seen as the distillation temperature
increases and is due to the evolution of this variable
to the nominal operating conditions. In this region a
thermal degradation of the emulsion takes place.
The second zone is observed when the distillation
temperature remains constant and is very close
to the theoretical boiling point of water at the
operating pressure.
Finally, the third zone occurs when the distillation
temperature increases with the percentage of distilled
liquid. In this zone the surface of the experimental
set-up becomes fouled and this is caused by thermal
cracking of the oil components.
The evolution of COD in the distillate with the
percentage of distilled liquid is represented in Figs 5
and 6 for the two wastes at the three different operating
pressures mentioned above.
, 700 mm Hg , 450 mm Hg , 300 mm Hg
Figure 5. COD evolution in the simple batch distillation of effluent 1.
, 700 mm Hg , 450 mm Hg , 300 mm Hg
Figure 6. COD evolution in the simple batch distillation of effluent 2.
536
In both of these cases two zones can be observed.
The first zone corresponds to the period in which the
amount of organic matter contained in the distillate
decreases dramatically to give COD levels below
2000 mg dm−3 . The second zone arises when the
COD begins to increase. On examining the normal
boiling points (from commercial data sheets) of the
components of both wastes it was found that all
components, with the exception of a demould agent
(DMA), have normal boiling points in excess of
250 ◦ C. DMA is an industrial reagent used to remove
the metallic material from the mould in the cast
process. This component has a normal boiling point
equal to that of water (ie 100 ◦ C) and is soluble in
water. The presence of this material in the waste
was also confirmed by gas chromatography with an
FID detector.
The normal boiling points of the components are
high (a difference of over 150 ◦ C in comparison to
water and DMA) and the oil and aqueous phases are
immiscible in both wastes. This situation allows the
first zone of the COD vs distilled percentage curve to
be interpreted as a binary liquid–vapour equilibrium
between water and DMA. Similarly, the second zone
can be considered as a region in which the aqueous
phase has been partially exhausted and oils begin to
distil due to the increase in temperature. This increase
in temperature is a consequence of problems with the
distillation of the aqueous phase. The breakdown of
the emulsion leads to two different phases; a lighter,
oily phase that is located above a heavier aqueous
phase. As the distillation progresses the higher oil
contents make it difficult for the aqueous phase
components to distil and, therefore, the temperature
begins to increase.
The increase in the initial COD values with pressure
in the first zone of the COD vs distilled percentage
curve is indicative of changes in the volatility of the
aqueous phase components. In order to confirm this,
the boiling points of water and DMA at different
pressures were measured (Fig 7). It can be observed
that both compounds have the same boiling point
at atmospheric pressure and that a decrease in the
operating pressure leads to a higher boiling point for
, water , DMA
Figure 7. Boiling points of water and DMA as a function of
operating pressure.
J Chem Technol Biotechnol 79:533–539 (online: 2004)
 Treatment of wastes from metalworking industries

DMA in comparison to water. This fact is indicative

of changes in the relative volatility and explains why
lower operating pressures lead to lower initial COD
values in the distillate.
The evolution of accumulated COD in the distillate
for the treatment of both wastes is shown in Figs 8
and 9. The COD decreases up to the point where
the distillation of 80–90% of the initial volume is
achieved. This point corresponds to the increase in
the distillation and cracking of oils.
The dependence of accumulated COD (at 85% of , effluent 1 , effluent 2
the initial volume of waste distilled) on the operating
pressure is represented in Fig 10. It can be observed Figure 10. Influence of operating pressure in resulting accumulated
COD (85% of the initial volume of water distilled).
that this parameter increases in a linear manner
with pressure, thus indicating that the best results
are obtained on working at lower pressures. This
behaviour can be explained by taking into account
the change in the relative volatility of water and DMA
discussed above.

3.3 Pilot plant-scale study

In an effort to confirm the results obtained in the
laboratory-scale study and to determine the influence
of scale-up, larger volumes (200 dm3 ) of the two
waste types under investigation were treated in
the batch pilot plant described in the experimental , effluent 1 , effluent 2

Figure 11. Evolution of accumulated COD with the percentage of

distilled waste volume in the pilot plant at 70 mm Hg.

Table 3. Scale-up comparison between results obtained in

laboratory-pilot plant-scale studies: accumulated COD for the
distillation of 85% of the waste volume

Effluent 1 Effluent 2

Extrapolation from data obtained in 1326 571

laboratory-scale study
Actual data obtained in the pilot 1250 520
plant-scale study
Error (%) 6.08 9.81
, 700 mm Hg , 450 mm Hg , 300 mm Hg

Figure 8. Accumulated COD (distillate) evolution in the simple batch

distillation of effluent 1. section. Bearing in mind the results obtained in
the liquid–vapour characterization study (ie low
operation pressures increase treated water quality),
it was decided to operate the distillation plant at the
minimum achievable working pressure (70 mm Hg).
The evolution of accumulated COD with the
percentage of distilled waste volume is shown in
Fig 11. As can be seen, similar results to those obtained
in the laboratory-scale study were obtained: the initial
zone corresponding to high COD due to distillation
of the demould agent was followed by a zone with
low COD and, subsequently, by the zone in which
distillation of oils occurred. As expected, the initial
COD values are lower than those measured in the
laboratory-scale study at higher pressures, although
, 700 mm Hg , 450 mm Hg , 300 mm Hg
these values are interrelated. The accumulated COD
Figure 9. Accumulated COD (distillate) evolution in the simple batch values (at 85% of the initial volume of waste distilled)
distillation of effluent 2. obtained for both waste flows are given in Table 3

J Chem Technol Biotechnol 79:533–539 (online: 2004) 537

P Cañizares et al
along with those predicted by extrapolation of the
laboratory-scale studies. It can clearly be seen that
the data match to an acceptable level, indicating that
scale-up factors do not influence the decontamination
process to any significant extent.
The discharge limit fixed by the relevant authority
dictates that the treatment must achieve a COD value
below 1500 mg dm−3 , since treated waste flows are
discharged to a municipal wastewater treatment plant.
From the results described above it is clear that more
than 90% of each waste flow can be distilled to achieve
these discharge limits. When oil distillation begins,
the temperature increases markedly and a simple
control system can be easily applied to automate
the batch distillation process and prevent the COD
increasing beyond the discharge limits. Thus, simple
batch distillation is a process that is technically suitable
for treatment of this type of waste.
3.4 Economic evaluation
The objective of the economic evaluation described
here is not to develop an exhaustive financial analysis.
Rather, the aim is to obtain an approximate estimate
of the capital investment and operating cost for the
treatment of the two effluents in question using
simple batch distillation, and to compare it with
corresponding treatment by a waste management
firm.
The estimation of cost depends on the scale
of the operation and so this analysis is focussed
on the particular case studied: a metalworking
factory that generates 800 m3 year−1 of effluent
1 and 200 m3 year−1 of effluent 2. Pre-design of
the plant (for economic evaluation purposes) was
carried out according to the experimental data
given in this paper. The study is based on a
simple batch distillation process that operates for
250 day year−1 , involves the use of several tanks
for the storage of the waste until treatment is
complete, and incorporates a filtration systems for
chip removal. The plant is assumed to be fully
automated.
An approximate estimate of the capital cost of the
whole plant was obtained by employing a multiple-
factor method.16 This method is based on an
evaluation of the price of the machinery and equipment
required for the plant (delivered to the plant), and
multiplying this cost by several factors that include the
cost contributions for each activity required to put the
waste treatment plant into operation.
The value of the machinery and equipment for this
process (reboiler, condenser, storage tanks, vacuum
pump etc) was estimated by obtaining individual
quotes (delivered to the plant) from several companies.
A value of 36 935 ¤ was determined for the overall cost
of machinery and equipment. The factors involved
in the calculation of the total capital investment are
shown in Table 4. From these values a total cost of
147 000 ¤ can be estimated for capital investment.
538
Table 4. Typical capital investment items
% of delivered
Item equipment
Equipment and machinery 100
Purchased equipment installation 76
Piping 33
Structural steel foundations, reinforced concrete 28
Electrical 9
Instruments 13
Battery-limits building and service 45
Total physical plant 304
Engineering supervision 41
Direct plant cost 345
Contractor’s fees, overheads 17
Contingency 36
Total fixed-capital investment 398
The operating costs can be evaluated by consid-
ering the following cost items: power, labour and
depreciation costs, treated waste discharge tax and
management of distillation residues as separate waste.
Power costs are estimated for a propane storage
heating system with a yield of 80%, assuming an
effluent temperature of 20 ◦ C, a boiling point of
approximately 44 ◦ C (at an operating pressure of
70 mm Hg) and a propane cost of 0.6 ¤kg−1 . The
labour cost is calculated assuming a labour rate of
20 ¤h−1 and 250 operating days year−1 . Since simple
batch distillation can be easily automated, labour
requirements are small and can be evaluated in units
of 1 h-labour day−1 .
The depreciation cost can be calculated on the
basis of the estimated capital cost, assuming that the
annual depreciation rate of the investment is 10%. The
residue resulting from the batch distillation process
(distillation bottoms) contains more than 50% of
oils. As a consequence, the calorific power of the
residue is very high (>3500 kcal kg−1 ) and its thermal
valorization must be considered. Unfortunately, the
small volume of bottoms generated (<100 m3 year−1 )
in this factory and the high quality requirements
for the combustion gases preclude this alternative.
The distillation bottoms must therefore be treated as
residues, a situation that adds a cost item to the process
(management of distillation bottoms). A typical cost
for this waste management is 150 ¤ m−3 . So, assuming
10% generation of these residues this item must be
evaluated in the order of 15000 ¤ year−1 .
Finally, the cost due to the discharge of treated
effluents can be estimated in terms of the distilled
fraction of effluents (90% of effluents) and assuming
a specific discharge tax of 0.30 ¤ m−3 . This results in
an annual cost of 270 ¤ year−1 .
The values of the different cost items are summa-
rized in Table 5. The resulting total cost is 51343.06 ¤
year−1 (51.34 ¤ m−3 ). It can be seen from the data in
Table 6 that the total cost, when compared with that
arising from the management of waste by a specialized
company (150 ¤ m−3 ), makes this a suitable alternative
J Chem Technol Biotechnol 79:533–539 (online: 2004)

from an economic viewpoint with a payback time of
only 1.30 years.
4 CONCLUSIONS
The main conclusions that can be drawn from this
work are:
(1) Distillation is a unit operation that can be
useful for the treatment of effluent generated in
metalworking factories, since the resulting wastes
consist mainly of oil-in-water emulsions and the
difference in the volatility of these two types of
compounds is significant. However, the presence
of numerous other compounds in this type of
industrial waste makes it necessary to carry out a
more detailed study of the technical feasibility of
the process in each particular case.
(2) The results obtained in the laboratory-scale
distillation of existing metalworking waste flows
indicate two different distillation regions. In the
first zone, organic matter contained in the distillate
decreases dramatically to give COD levels below
2000 mg dm−3 . A second zone is then observed in
which the COD begins to increase. The normal
boiling points of the components are high (a
difference of over 150 ◦ C with respect to water
and DMA) and the oil and aqueous phases
are immiscible in both types of waste. It can
therefore be concluded that the first zone of the
COD vs distilled percentage curve is a binary
liquid–vapour equilibrium between water and
DMA, and the second zone is a region in which
the aqueous phase has been partially exhausted
and oils begin to distil as a consequence of the
increase in temperature.
(3) Simple batch distillation is a process that
is technically suitable for the treatment of
the effluents described here. Scale-up factors
do not greatly influence the results obtained
in the decontamination process. Temperature
Table 5. Estimated operating costs for the distillation treatment of the
two effluents
Total capital investment (¤)
Depreciation of investment (¤ year−1 )
Power requirement (¤ year−1 )
Labour cost (¤ year−1 )
Management of remainders (¤ year−1 )
Dumping of treated effluents (¤ year−1 )
Operating cost (¤ year−1 )
Table 6. Comparison of treatment alternatives
Alternative Cost (¤ year−1 )
Waste management
Treatment by means of distillation
Benefit
J Chem Technol Biotechnol 79:533–539 (online: 2004)
Treatment of wastes from metalworking industries
differences in the distillation make this process
easy to automate.
(4) Distillation is a suitable alternative from an
economic viewpoint compared with effluent
treatment by a waste management firm; the
payback time associated with distillation is only
1.30 years and a benefit of 98.66 ¤ m−3 of treated
effluent is calculated.
ACKNOWLEDGEMENTS
This work was supported by the JCCM (Junta de
Comunidades de Castilla La Mancha) through the
project PC-02-002 ‘‘Gestión Integral del Agua en
Industrias de Fundición y Mecanizado de Metales’’.
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